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The synthesis and structural characterization of a series of homoleptic cobalt complexes of general formula [Co(R-pyX) 3 ] is reported, where X ϭ S, Se; R ϭ H, 3-CF 3 and 5-CF 3 . The compounds were synthesized by electrochemical oxidation of the metal in a cell containing an acetonitrile solution of the corresponding ligand. When 2,2Ј-bipyridine (bipy) or 1,10-phenanthroline (phen) were added to the electrolytic cell, mixed cobalt(II) compounds [Co(R-pyX) 2 L] (L ϭ bipy, phen) were also isolated. All of the complexes obtained have been characterized by microanalysis, vibrational and electronic spectroscopy, FAB mass spectrometry * Professor Dr. M. L. Durán 1853 and, in the case of diamagnetic compounds that were sufficiently soluble, by 1 H and 13 C NMR spectroscopy. Crystals of [Co(3-CF 3 -pyS) 3 ] and [Co(5-CF 3 -pyS) 3 ] were obtained and studied by X-ray diffraction. The crystal structures consist of monomeric molecules with the metal atom in an octahedral environment and the ligands in a meridional disposition.